Trifluoroacetic acid → n-(4-Amino-3-methylphenyl) {[(5-chloro(2-thienyl))sulfonyl]amino}-carboxamide

HRID 1071734ノート

反応式

HRID 1071734 の反応式
C(OC([NH:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([NH:18][S:19]([C:22]2[S:23][C:24]([Cl:27])=[CH:25][CH:26]=2)(=[O:21])=[O:20])=[O:17])=[CH:11][C:10]=1[CH3:28])=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([NH:18][S:19]([C:22]2[S:23][C:24]([Cl:27])=[CH:25][CH:26]=2)(=[O:21])=[O:20])=[O:17])=[CH:11][C:10]=1[CH3:28]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 22064442N-(4-[(tert-butoxy)carbonylamino]-3-methylphenyl}{[(5-chloro(2-thienyl))sulfonyl]amino}carboxamide

生成物 1

HCID 22064409n-(4-Amino-3-methylphenyl) {[(5-chloro(2-thienyl))sulfonyl]amino}-carboxamide収率 136.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a chilled solution of N-{4-[(tert-butoxy)carbonylamino]-3-methylphenyl}{[(5-chloro(2-thienyl))sulfonyl]amino}carboxamide (0.246 g, 0.55 mmol) in CH2Cl2 (5 mL) was added neat TFA (1.1 mL). The reaction mixture was stirred cold for 1.5 hr, concentrated in vacuo, azeotroped with heptane and dried to give N-(4-amino-3-methylphenyl){[(5-chloro(2-thienyl))sulfonyl]amino}-carboxamide (0.26 g) as the mono TFA salt. ES-MS (M+H)+=346.

後処理

  1. concentrationconcentrated in vacuo
  2. customazeotroped with heptane
  3. customdried

出典と根拠

ORDレコード
ord-c90809dcaf9d4c3fbdd51069d4ec529a
出典データセット
uspto-grants-2005_06
特許番号
US06906063B2

反応ノート

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